Metal Oxide Combinatorial
Synthesis and Characterization
Yaniv Bouhadana
Simcha Meir
Assaf Anderson
Sven Rühle
Arie Zaban
Eli Rosh-Hodesh
Hannah-Noa Barad
Institute for Nanotechnology & Advanced Materials
Bar Ilan Universtiy, Ramat Gan 52900
yaniv.phd@gmail.com
What is Our Main Goal?
Cheng, F., & Chen, J. (2012).. Chemical Society reviews, 41(6), 2172–92.
We want to find an efficient,
durable, low cost electro-catalyst
for metal air batteries
Methodology
Combinatorial Material
Science
Metal Oxides
Combinatorial
Synthesis
• Data Mining, DOE,
Computational Chemistry
Based on our parallel research in All-Oxide PV.
Data Mining
Data Analysis
• High Throughput
Analysis Methods
Analysis
Analysis
• High Throughput
Synthesis Methods
Synthesis

• Combinatorial Research
Concepts
Combinatorial
Outlines
Synthesis
 long term stability
Combinatorial
Why Oxides?
Low Cost synthesis/fabrication
Data Mining
Abandon materials
Analysis
Non-hazardous materials
Abundance of Elements
Combinatorial
Combinatorial Material Science - Concept
Synthesis
Analysis
Data Mining
Combinatorial
Combinatorial Material Science
Synthesis
Analysis
Data Mining
 60 “useful” elements which are the constituents of
 60
x 60 = 3600 binary compounds (A-B, still not includes AxB,
 60
x 60 x 60 = 216,000 ternary compounds (A-B-C…) 
ABx etc..)  most known
Synthesis
 ~30.000 inorganic compounds
Combinatorial
Combinatorial Material Science
~3% known
Analysis
Data Mining
High TC Superconductors
Combinatorial
Proof of Concept:
Synthesis
Analysis
Data Mining
Combinatorial
New Composite Oxides
Synthesis
Analysis
new
new
crystalline amorphous
phase
phase
polycrystalline
composite material – bifunctional catalysts.
Data Mining
low impurity
concentration
(doping)
Combinatorial
Combinatorial Material Science
Synthesis
Analysis
Data Mining
The Ultimate Oxide
Electro Catalist
Materials
Combinatorial
Combinatorial Synthesis Methods
Synthesis
Spray Pyrolysis
Pulse Laser Deposition
Analysis
(+Multi-Source Sputtering)
Data Mining
Pulsed Laser Deposition
Combinatorial
Combinatorial Synthesis Methods
Continuous Compositional Spread (CCS)
Synthesis
Analysis
Data Mining
SrTiO3 + Co3O4
Combinatorial
Composite Oxide
Synthesis
Co3O4
Data Mining
Co3O4
Analysis
Jsc
SrTiO3
Jsc
 Scanning Optical Characterization
 Scanning Electric Conductivity
 Scanning X-Ray Diffraction (soon)
Data Mining
 Scanning Seebeck Effect (planned)
Analysis
 Scanning Profilometer
Synthesis
 Scanning Electrochemical Characterization
Combinatorial
Large Throughput Analysis




BioLogic Potentiostat (includes FRA Module)
Tango XYZ table.
Perestaltic Punp (RS485/232 controled).
Silent vacume pump + solution trup.
 Special smaple holder (secured).
 Spacial surface Portable electrocemical cell.
 Tubing.
 Operating softwere.
 Analisys softwere.
Data Mining
Softwere:
Analysis
Mechanics:
Synthesis
Electronics:
Combinatorial
Scanning Electrochemical Meas.
Synthesis
Analysis
At the initial stage the
measurement that is
preformed in the
electrochemical
scanner is cyclic
voltammetry and the
percentage of oxygen
is constant.
Combinatorial
Electrochemical Scan Procedure
Data Mining
Combinatorial
Scanning Electrochemical Meas.
foil : preferred – platina foil,
current – stainless steel.
Solution In
Ref
Counter
Synthesis
Portable electrochemical cell
• 3 Electrodes Cell:
– Counter : any metallic
– Working : the
Analysis
combinatorial samples
bases on FTO.
– Reference : Ag/AgCl
(Kalomel) , PdS
K3Fe(CN)6/K4Fe(CN)6/KCl
Solution
Out
Data Mining
Electrolyte : Polysulfide,
designed by Dr. Assaf Anderson
Combinatorial
Scanning Optical Characterization
Synthesis
Analysis
What can we extract?
 absorption coefficient
 thickness
 band gap
Data Mining
What do we measure?
 Total Transmission
 Total Reflection
 Specular Reflection
 350 – 1100 nm
d(x,y) = d0 · cosnx(x-x0) · cosny(y-y0)
Combinatorial
Scanning Profilometer
Synthesis
Analysis
Data Mining
What can we extract?
 conductivity σ / resistivity ρ
 thickness
 activation energies (planned)
Synthesis
What do we measure?
 I-V curve (2 point or 4 point contact)
 temperature dependent (planned)
Combinatorial
Scanning Conductivity
Analysis
Data Mining
Example: Resistance of ZnO with linear
thickness gradient
(planned)
What can we extract?
 Seebeck coefficient
 type of doping (n or p)
Synthesis
What do we measure?
 Voltage
Combinatorial
Scanning Seebeck Effect Meas.
Heater
Analysis
Seebeck Coefficient
Data Mining
SA, SB = Thermopower or
Combinatorial
Scanning X-Ray Diffraction
Synthesis
Analysis
Data Mining
What can we extract?
 phase analysis, structural data
Synthesis
SnO2
Combinatorial
Presentation of Results
Analysis
Data Mining
Combinatorial
Database and Data Mining
Synthesis
Analysis
Data Mining
Combinatorial
Database and Data Mining
Synthesis
Analysis
Data Mining
The Ultimate Oxide
Electro Catalist
Materials
 Combinatorial Material Science – Concept
 Combinatorial Synthesis Methods
 Spray Pyrolysis/ PLD
Synthesis
 Let’s look into the unknown
Combinatorial
Summary
 High Throughput Analysis
electrochemical , etc.
Analysis
 optical, conductivity, profilometer,
Data Mining and Theoretical Chemistry
predict our next research items.
Data Mining
 Proof of Concept, lookout for trendlines and
Thank you for your attention!
Yaniv.phd@gmail.com